CN111943668A - Medium-temperature sintered high-dielectric low-loss negative temperature compensation type porcelain and preparation method thereof - Google Patents

Medium-temperature sintered high-dielectric low-loss negative temperature compensation type porcelain and preparation method thereof Download PDF

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CN111943668A
CN111943668A CN202010631800.9A CN202010631800A CN111943668A CN 111943668 A CN111943668 A CN 111943668A CN 202010631800 A CN202010631800 A CN 202010631800A CN 111943668 A CN111943668 A CN 111943668A
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CN111943668B (en
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刘杨琼
李红卫
黄振娟
汪小玲
赵杨军
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Chengdu Hongke Electronic Technology Co ltd
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Abstract

The invention belongs to the technical field of ceramic materials, and provides a medium-temperature sintered high-dielectric low-loss negative temperature compensation type porcelain and a preparation method thereof. The high-dielectric-medium low-loss negative temperature compensation type porcelain comprises raw materials including a base material, a modifier and a sintering aid; the chemical formula of the base material is Sr1‑xBixTiO3Wherein x is more than or equal to 0.14 and less than or equal to 0.18; the modifier comprises CaCO3And Re2O3The sintering aid comprises ZnO and ZnO-B2O3And (3) glass. The negative temperature compensation type porcelain has a dielectric constant of more than or equal to 900 and can be used for preparing a capacitor with a smaller size; dielectric loss less than or equal to 4.8 multiplied by 10‑4The heating caused by loss can be reduced, and the service life is prolonged; the material can be sintered at a medium temperature, so that the energy consumption is low and the production cost is saved; resistance to impulseStrong, can be used in alternating current or pulse working environment. The preparation method obtains the product by sintering at medium temperature through a solid-phase synthesis method. The preparation method has simple process and is easy for industrialized production.

Description

Medium-temperature sintered high-dielectric low-loss negative temperature compensation type porcelain and preparation method thereof
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation type porcelain and a preparation method thereof.
Background
At present, the large-capacity ceramic capacitor of the DC/DC power supply module and the EMI filter adopts X7R material mostly. However, X7R material has large AC loss (tan ≥ 0.025), and when it is operated by AC or pulse, it will generate heat and raise temperature to generate micro-crack, thus resulting in failure.
The negative temperature compensation type porcelain has the advantages of high dielectric constant, low loss and the like, and combines the most advantageous dielectric properties of NPO and X7R under the condition of-55 to +125 ℃. The method has high reliability, is mainly used for preparing high-voltage pulse alternating-current low-loss SMD type MLCC products of AC/DC and DC/DC modules, and is widely applied to electronic equipment matched with military major engineering of national defense, aviation, aerospace and the like.
At present, the more researched negative temperature compensation type dielectric material is CaTiO3、SrTiO3、TiO2、CaZrO3. In which CaTiO3、TiO2、CaZrO3The dielectric constant at room temperature of 150, 100 and 40 respectively, the dielectric constant is low, and the characteristic of high dielectric constant is difficult to realize. SrTiO3The base ceramic has low Curie temperature (about-250 deg.C), relatively high dielectric constant (about 270) at normal temperature, paraelectric state, and low loss (dielectric loss up to 10)-3-10-4) And is one of the most interesting materials.
However, since SrTiO3The dielectric constant of the base ceramic is still at a lower level, miniaturization is difficult to realize, and the problem of loss heating failure mechanism under the existing pulse and alternating current work is difficult to solve. Therefore, how to maintain SrTiO3Under the advantages of the paraelectric state and low loss of the base ceramic, the dielectric constant of the base ceramic can be further improved, which is a problem to be solved at present.
Disclosure of Invention
Aiming at the defects in the prior art, the first purpose of the invention is to provide a medium-temperature sintered high-dielectric low-loss negative temperature compensation type porcelain; the negative temperature compensation porcelain has dielectric constant of not less than 900, and can be used for preparing smaller porcelainThe capacitor of (1); dielectric loss less than or equal to 4.8 multiplied by 10-4The heating caused by loss can be reduced, and the service life is prolonged; the material can be sintered at a medium temperature, so that the energy consumption is low and the production cost is saved; the pulse resistance is strong, and the device can be used in alternating current or pulse working environments.
Aiming at the defects in the prior art, the second purpose of the invention is to provide a preparation method of a medium-temperature sintered high-dielectric low-loss negative temperature compensation type porcelain material; the preparation method has simple process and is easy for industrialized production.
In order to achieve the above purpose, the solution adopted by the invention is as follows:
a medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation porcelain comprises raw materials of a base material, a modifier and a sintering aid; the chemical formula of the base material is Sr1-xBixTiO3Wherein x is more than or equal to 0.14 and less than or equal to 0.18; the modifier comprises CaCO3And Re2O3The sintering aid comprises ZnO and ZnO-B2O3And (3) glass.
A preparation method of the medium-temperature sintered high-dielectric low-loss negative temperature compensation type porcelain comprises the following steps: (1) sr is1- xBixTiO3、CaCO3ZnO and ZnO-B2O3Mixing the glass according to the proportion, ball-milling, drying, sieving, and calcining at the temperature of 1060 +/-20 ℃ to obtain a required clinker; (2) then adding Re into the calcined clinker according to the mixture ratio2O3Ball milling, drying and sieving to obtain porcelain; (3) and pressing the ceramic powder into a sheet, heating to 1120-1160 ℃ after removing the gel, sintering for 3-4h, cooling along with the furnace to obtain a ceramic wafer, coating the surface of the wafer and firing an electrode for testing the performance of the wafer.
The invention provides a medium-temperature sintered high-dielectric low-loss negative temperature compensation type porcelain and a preparation method thereof, which have the beneficial effects that:
(1) the invention provides a medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation type porcelain, which comprises the raw materials of a base material, a modifier, a sintering aid and a cooling agent. Wherein the chemical formula of the base material is Sr1-xBixTiO3The base material is introduced into SrTiO3Adding inBi3+To increase its dielectric constant and by modifying CaCO3And Re2O3Doping modification is carried out to cause lattice distortion, the linear change can be kept between-55 ℃ and +125 ℃ in the use temperature range, the paraelectric state of the room temperature is kept unchanged, and small dielectric loss is maintained; re2O3The doping can play a role in further reducing the dielectric loss of the material; in the preparation process of the clinker, a sintering aid ZnO is added to improve the calcination efficiency, and a glass material ZnO-B is directly added2O3The wetting and coating functions of the glass can directly reduce the calcining temperature of the clinker. The glass material is directly added in the preparation process of the clinker, so that the purpose of medium-temperature sintering by adding a small amount of glass can be achieved, and the production cost is saved. The raw materials can cooperate with each other to jointly achieve the purposes of improving the dielectric constant of the product, reducing the dielectric loss and realizing medium-temperature sintering by adding a small amount of glass.
(2) The preparation method of the medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation type porcelain material comprises the steps of fully mixing the raw materials by adopting a solid-phase synthesis method, increasing the contact area between the compounds, and facilitating the diffusion of atoms or ions so as to increase the synthesis rate; by simultaneously regulating and controlling the range ratio of the materials, the balls and the water in the synthesis process, the ball milling time and the calcining temperature, the ceramic material which has high reliability and meets the dielectric property required by the application can be prepared. In this application, Re2O3The calcined briquette is subjected to secondary doping modification synthesis, so that the aim of reducing dielectric loss is further fulfilled.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a detailed description of a medium-temperature sintered high-dielectric low-loss negative temperature compensation porcelain and a preparation method thereof provided by the embodiments of the present invention.
A medium-temperature sintered high-dielectric-index low-loss negative temperature compensation porcelain comprises a base material, a modifier and a sintering aid. The chemical formula of the base material is Sr1-xBixTiO3Wherein x is more than or equal to 0.14 and less than or equal to 0.18; the modifier comprises CaCO3And Re2O3. Wherein, Re2O3Can serve to further reduce dielectric loss.
In this embodiment, Sr can be substituted by1-xBixTiO3The doping modifier causes lattice distortion, shifts Curie temperature to the normal temperature direction, improves dielectric constant, keeps linear change within the using temperature range (-55 ℃ to +125 ℃), keeps the cis-state of room temperature unchanged, and maintains small dielectric loss.
In this example, CaCO3Is composed of Sr1-xBixTiO3In a molar percentage of 5 to 8 mol%, Re2O3Is composed of Sr1- xBixTiO3The mass percentage of (B) is 0.21-0.61 wt%. The modifier further comprises BaCO3And MnCO3(ii) a Wherein, BaCO3Is composed of Sr1-xBixTiO3Less than or equal to 4 mol%, MnCO3 is Sr1-xBixTiO3Is less than or equal to 0.03 wt%.
The sintering aid comprises ZnO and ZnO-B2O3And (3) glass. Wherein ZnO accounts for Sr1-xBixTiO3Is 1.5-3 mol%. ZnO-B2O3Glass is composed of Sr1-xBixTiO3The mass percentage of the component (B) is 0.2-0.75 wt%.
ZnO-B2O3The glass further comprises 75-85 wt% of ZnO and 15-25 wt% of B2O3. In the range of the mixture ratio, ZnO-B2O3Glass pair Sr1-xBixTiO3Has better wetting and coating effectsAnd the purpose of cooling is easily achieved. Further, in this example, ZnO-B2O3The glass consists of ZnO and B2O3Ball milling and mixing, and sintering at 800-870 deg.c. In this temperature range, ZnO-B2O3And a continuous glass structure is easier to form, and the phenomenon that the glass phase cannot be formed due to too low temperature and the hardness is too high due to too high temperature is avoided.
The embodiment of the invention also provides a preparation method of the medium-temperature sintered high-dielectric low-loss negative temperature compensation type porcelain, which comprises the following steps: (1) sr is1-xBixTiO3、CaCO3、BaCO3ZnO and ZnO-B2O3Glass is loaded into a hopper according to the proportion, and the weight ratio is as follows: ball: water 1: 5: (2-2.5) performing ball milling for 6-8h, drying, sieving, and calcining at (1060 +/-20) DEG C to obtain a required clinker; (2) adding MnCO into the calcined clinker according to the proportion3And Re2O3According to materials: ball: water 1: 5: (1-1.5) ball-milling for 24-30h, drying and sieving to obtain the required porcelain; (3) adding 7-12 wt% of paraffin wax into the porcelain material for granulation, pressing into a wafer, then increasing the temperature to 450 ℃ at the speed of 2 ℃/min, discharging the adhesive, then increasing the temperature to 1120-.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of a medium-temperature sintered high-dielectric-medium low-loss negative temperature compensation type porcelain, which comprises the following steps: (1) taking x as 0.15, adding Sr1-xBixTiO3Is composed of1-xBixTiO3Of 6 mol% of CaCO3Is composed of1- xBixTiO3The mol percent of ZnO is 2mol percent and the Sr is1-xBixTiO30.75 wt% of ZnO-B2O3Glass is loaded into a hopper according to the proportion, and the weight ratio is as follows: ball: water 1: 5: 2 for 8 hours, drying and sieving,then calcining at 1080 ℃ to obtain a required clinker; (2) adding Sr into the calcined clinker according to the proportion1-xBixTiO30.03 wt% of MnCO3And is accounted for Sr1-xBixTiO30.21 wt% of Re2O3According to materials: ball: water 1: 5: 1, ball-milling for 30 hours, drying and sieving to obtain the required porcelain; (3) adding 7-12 wt% of paraffin wax into the porcelain material for granulation, pressing into a wafer, then increasing the temperature to 450 ℃ at the speed of 2 ℃/min, discharging the adhesive, then increasing the temperature to 1120-.
Example 2
The embodiment provides a preparation method of a medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation type porcelain, which can refer to embodiment 1 and is different from that: in step (1), Sr is added1-xBixTiO3Is composed of1-xBixTiO3Of 8 mol% of CaCO3Is composed of1-xBixTiO3Has a molar percentage of 3mol percent ZnO and Sr1-xBixTiO30.3 wt% of ZnO-B2O3Glass is loaded into a hopper according to the proportion; in the step (2), Sr is added into the calcined clinker according to the proportion1-xBixTiO30.11 wt% of Re2O3。
Example 3
The embodiment provides a preparation method of a medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation type porcelain, which can refer to embodiment 1 and is different from that: in step (1), Sr is added1-xBixTiO3Is composed of1-xBixTiO3Of 5 mol% of CaCO3Is composed of1-xBixTiO3Is 1.5 mol% of ZnO and accounts for Sr1-xBixTiO30.35 wt% of ZnO-B2O3Glass buttonProportionally loading into a hopper; in the step (2), Sr is added into the calcined clinker according to the proportion1-xBixTiO30.61 wt% of Re2O3。
Example 4
The embodiment provides a preparation method of a medium-temperature sintered high-dielectric-medium low-loss negative temperature compensation type porcelain, which comprises the following steps: (1) taking x as 0.16, adding Sr1-xBixTiO3Is composed of1-xBixTiO3Of 6 mol% of CaCO3Is composed of1- xBixTiO3Of 2 mol% of BaCO3Is composed of1-xBixTiO3The mol percent of ZnO is 2mol percent and the Sr is1-xBixTiO30.5 wt% of ZnO-B2O3Glass is loaded into a hopper according to the proportion, and the weight ratio is as follows: ball: water 1: 5: 2.5, performing ball milling for 6 hours, drying, sieving, and calcining at 1040 ℃ to obtain a required briquette; (2) adding Sr into the calcined clinker according to the proportion1-xBixTiO30.03 wt% of MnCO3And is accounted for Sr1-xBixTiO30.29 wt% of Re2O3According to materials: ball: water 1: 5: ball milling for 24h according to the proportion of 1.5, drying and sieving to obtain a ceramic product; (3) adding 7-12 wt% of paraffin wax into the porcelain material for granulation, pressing into a wafer, then increasing the temperature to 450 ℃ at the speed of 2 ℃/min, discharging the adhesive, then increasing the temperature to 1120-.
Example 5
The embodiment provides a preparation method of a medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation type porcelain, which can refer to embodiment 4 and is different from that: in step (1), Sr is added1-xBixTiO3Is composed of1-xBixTiO3Of 6 mol% of CaCO3Is composed of1-xBixTiO3The mol percent of ZnO is 2mol percent and the Sr is1-xBixTiO30.5 wt% of ZnO-B2O3Glass is loaded into a hopper according to the proportion; in the step (2), Sr is added into the calcined clinker according to the proportion1-xBixTiO30.24 wt% of Re2O3。
Example 6
The embodiment provides a preparation method of a medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation type porcelain, which can refer to embodiment 4 and is different from that: in step (1), Sr is added1-xBixTiO3Is composed of1-xBixTiO3Of 6 mol% of CaCO3Is composed of1-xBixTiO3BaCO of 4 mol%3Is composed of1-xBixTiO3The mol percent of ZnO is 2mol percent and the Sr is1-xBixTiO30.5 wt% of ZnO-B2O3Glass is loaded into a hopper according to the proportion; in the step (2), Sr is added into the calcined clinker according to the proportion1-xBixTiO30.03 wt% of MnCO3And is accounted for Sr1-xBixTiO30.49 wt% of Re2O3。
Example 7
The embodiment provides a preparation method of a medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation type porcelain, which can refer to embodiment 4 and is different from that: in step (1), Sr is added1-xBixTiO3Is composed of1-xBixTiO3Of 6 mol% of CaCO3Is composed of1-xBixTiO3The mol percent of ZnO is 2mol percent and the Sr is1-xBixTiO30.4 wt% of ZnO-B2O3Glass is loaded into a hopper according to the proportion; in the step (2), Sr is added into the calcined clinker according to the proportion1-xBixTiO30.56 wt% of Re2O3。
Example 8
The embodiment provides a preparation method of a medium-temperature sintered high-dielectric-medium low-loss negative temperature compensation type porcelain, which comprises the following steps: (1) taking x as 0.17, adding Sr1-xBixTiO3Is composed of1-xBixTiO3Of 7 mol% of CaCO3Is composed of1- xBixTiO3Of 1 mol% of BaCO3Is composed of1-xBixTiO3Has a molar percentage of 2.5 mol% ZnO and Sr1-xBixTiO30.4 wt% of ZnO-B2O3Glass is loaded into a hopper according to the proportion, and the weight ratio is as follows: ball: water 1: 5: 2.3, performing ball milling for 7 hours, drying, sieving, and calcining at 1050 ℃ to obtain a required briquette; (2) adding Sr into the calcined clinker according to the proportion1-xBixTiO30.49 wt% of Re2O3According to materials: ball: water 1: 5: ball milling for 28h according to the proportion of 1.3, drying and sieving to obtain a ceramic product; (3) adding 7-12 wt% of paraffin wax into the porcelain material for granulation, pressing into a wafer, then increasing the temperature to 450 ℃ at the speed of 2 ℃/min, discharging the adhesive, then increasing the temperature to 1120-.
Example 9
The embodiment provides a method for preparing a medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation type porcelain, which can refer to embodiment 8, and is different from the following steps: in step (1), Sr is added1-xBixTiO3Is composed of1-xBixTiO3Of 6 mol% of CaCO3Is composed of1-xBixTiO3The mol percent of ZnO is 2mol percent and the Sr is1-xBixTiO30.2 wt% of ZnO-B2O3Glass is loaded into a hopper according to the proportion; in step (2), calciningSr is added into the baked blocks according to the proportion1-xBixTiO30.02 wt% of MnCO3And is accounted for Sr1-xBixTiO30.29 wt% of Re2O3。
The formulation for examples 1-9 is given in table 1:
TABLE 1
Figure BDA0002569197060000091
Experimental example 1
The experimental method comprises the following steps: the high-dielectric-constant low-loss negative temperature compensation type porcelain prepared in the embodiments 1 to 9 is tested for dielectric constant by an Agilient8722ET network analyzer (the dielectric constant is measured by the following steps ofr) Dielectric loss factor (tg) and temperature coefficient of capacity (α)c) The test results are shown in table 2:
TABLE 2
Figure BDA0002569197060000092
Figure BDA0002569197060000101
As can be seen from the data in Table 2, the high-dielectric low-loss negative temperature compensation type porcelain prepared by the preparation method of the embodiments 1-9 has a dielectric constant of 900 or more and a dielectric loss of 4.8 × 10 or less-4The temperature coefficient of the capacity can reach the KL group of-2200 +/-500 ppm/DEG C in the national standard, and the dielectric ceramic product does not contain harmful substances such as lead and the like and accords with the RoHS instruction; the sintering temperature 1120-1160 ℃.
In conclusion, the high-dielectric low-loss negative temperature compensation porcelain provided by the invention is adopted; the negative temperature compensation type porcelain has a dielectric constant of more than or equal to 900 and can be used for preparing a capacitor with a smaller size; dielectric loss less than or equal to 4.8 multiplied by 10-4The heating caused by loss can be reduced, and the service life is prolonged; the material can be sintered at medium temperature, so that the energy consumption is low and the production cost is saved; pulse resistanceThe performance is strong, and the device can be used in alternating current or pulse working environment; the preparation method has simple process and is easy for industrialized production.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A medium-temperature sintered high-dielectric low-loss negative temperature compensation porcelain is characterized in that: the raw materials comprise a base material, a modifier and a sintering aid; the chemical formula of the base material is Sr1-xBixTiO3Wherein x is more than or equal to 0.14 and less than or equal to 0.18; the modifier comprises CaCO3And Re2O3The sintering aid comprises ZnO and ZnO-B2O3And (3) glass.
2. The medium-temperature sintered high-dielectric-medium low-loss negative temperature compensation porcelain according to claim 1, which is characterized in that: the CaCO3Is composed of said Sr1-xBixTiO3In a molar percentage of 5 to 8 mol%, the Re2O3Is composed of said Sr1-xBixTiO3Is 0.21 to 0.61wt percent, and the ZnO accounts for the Sr1-xBixTiO3The mol percent of the ZnO-B is 1.5-3mol percent2O3Glass occupies the Sr1-xBixTiO3The mass percentage of the component (B) is 0.2-0.75 wt%.
3. The medium-temperature sintered high-dielectric-medium low-loss negative temperature compensation porcelain according to claim 2, which is characterized in that: the modifier also comprises BaCO3(ii) a The BaCO3Is composed of said Sr1-xBixTiO3Is less than or equal to 4 mol%.
4. Medium temperature firing according to claim 2 or 3The high-dielectric low-loss negative temperature compensation porcelain of the junction is characterized in that: the modifier also comprises MnCO3(ii) a The MnCO3Is composed of said Sr1-xBixTiO3Is less than or equal to 0.03 wt%.
5. The medium-temperature sintered high-dielectric-medium low-loss negative temperature compensation porcelain according to claim 2, which is characterized in that: the ZnO-B2O3The glass comprises: 75-85 wt% of ZnO and 15-25 wt% of B2O3。
6. The medium-temperature sintered high-dielectric-medium low-loss negative temperature compensation porcelain according to claim 5, which is characterized in that: the ZnO-B2O3The glass consists of ZnO and B2O3Ball milling and mixing, and sintering at 800-870 deg.c.
7. A method for preparing medium-temperature sintered high-dielectric-constant low-loss negative temperature compensation porcelain according to claim 4, which is characterized in that: the method comprises the following steps:
(1) subjecting said Sr to1-xBixTiO3The CaCO3The ZnO and the ZnO-B2O3Mixing the glass according to the proportion, ball-milling, drying, sieving, and calcining at the temperature of 1060 +/-20 ℃ to obtain a required clinker;
(2) adding Re into the calcined clinker according to the mixture ratio2O3Ball milling, drying and sieving to obtain porcelain;
(3) pressing the ceramic material into a wafer, heating to 1120-1160 ℃ after removing the gel, sintering for 3-4h, cooling along with a furnace to obtain a ceramic wafer, coating the surface of the wafer and firing an electrode for testing the performance of the wafer.
8. The preparation method of the medium-temperature sintered high-dielectric-medium low-loss negative temperature compensation type porcelain according to claim 7, characterized in that: in the step (1), the Sr filling step is further included1-xBixTiO3Mole ofBaCO in a percentage of less than or equal to 6 mol%3。
9. The preparation method of the medium-temperature sintered high-dielectric-medium low-loss negative temperature compensation type porcelain according to claim 7, characterized in that: in the step (1), the method also comprises the step of filling the MnCO into the clinker3。
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